CN102182056A - Method for preparing titanium dioxide nanoparticle composite silver plating on surface of polyester fabric - Google Patents
Method for preparing titanium dioxide nanoparticle composite silver plating on surface of polyester fabric Download PDFInfo
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- CN102182056A CN102182056A CN 201110125514 CN201110125514A CN102182056A CN 102182056 A CN102182056 A CN 102182056A CN 201110125514 CN201110125514 CN 201110125514 CN 201110125514 A CN201110125514 A CN 201110125514A CN 102182056 A CN102182056 A CN 102182056A
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Abstract
The invention discloses a method for preparing a titanium dioxide nanoparticle composite silver plating on the surface of a polyester fabric. The method comprises the following steps: firstly preprocessing the polyester fabric; and secondly preparing the titanium dioxide nanoparticle composite silver plating on the surface of the polyester fabric. The method has the following beneficial effects: based on the traditional chemical silver plating process, aiming at the defect of high possibility of agglomeration of the titanium dioxide nanoparticles, a dispersing agent is used for carrying out ultrasonic dispersion on the titanium dioxide nanoparticles and then the titanium dioxide nanoparticles are added to the chemical silver plating solution to carry out titanium dioxide nanoparticle composite chemical silver plating on the polyester fabric under the condition of ultrasonic waves, thus not only improving the wear resistance of the chemical silver plated polyester fabric but also endowing the chemical silver plated fabric with photocatalytic activity.
Description
Technical field
The invention belongs to exploitation of nano material and electroless plating technology and applied technical field, relate to a kind of surface modifying method of dacron, be specifically related to a kind of method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle.
Background technology
Along with the fast development of household electrical appliance such as mobile phone, computer and micro-wave oven and extensively universal, the harm of electromagenetic wave radiation becomes increasingly conspicuous.Explore the particularly flexible electromagnetic wave screen fabric of high-efficiency electromagnetic shielding material, prevent electromagnetic interference that electromagnetic wave causes, electromagnetic compatibility and, guarantee that the safe and smooth and personal safety of information communication system, network system and transmission system etc. has crucial meaning the injury of human body.Chemical silvering fabric quality is frivolous, and soft ventilative, anti-corrosion antibiotic, shielding electromagnetic wave is safe and reliable, can be widely used in the anti-electromagnetic radiation field.On fabric, carry out chemical silvering at present, main formaldehyde or reducing sugar and the silver-colored ammion complex salt generation redox reaction of adopting, at fiber surface deposition layer of metal silver, because chemical silvering is not self-catalyzed reaction, each plating only can be plated skim, therefore coating is deep not enough, and performance does not reach requirement, and the coating fastness is relatively poor.Nano titanium oxide is as a kind of important semi-conducting material, have nontoxic, be difficult for taking place advantage such as photochemical corrosion, aspect photocatalytic degradation is removed pollutant in the environment, bringing into play more and more important effect; Titanic oxide material also is a kind of novel anti-biotic material simultaneously, is widely used in the fiber product.In chemical plating liquid, add titanium dioxide nanoparticle, use the ultrasonic wave auxiliary process, not only can increase the thickness of chemical plating silver layer, and can make silver coating fabric obtain the photocatalytic degradation performance.
Using titanium dioxide nanoparticle that dacron is carried out chemically composited silver-plated correlation technique does not at present also have.Existing chemical plating nickel-phosphorus alloy preparation process of textile, the general nano particle that adopts has zinc oxide, carborundum and tin ash, use sodium alginate soln to carry out ultrasonic dispersion as dispersion liquid, and then nano dispersion fluid added in the chemical nickel phosphorus plating liquid, prepare nano particle composite nickel-plating phosphorus fabric, nanoparticulate dispersed is bad in the plating bath, nano particle can not be individual particle and be dispersed in the plating bath, therefore coating and fibrous matrix are bad in conjunction with fastness, have had a strong impact on the wear-resisting and washing durability of chemical nickel phosphorus plating fabric.
Summary of the invention
The purpose of this invention is to provide a kind of method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle, the general chemistry silver coating fabric silvering that has solved existing method preparation is thinner, does not have the problem of photocatalytic degradation performance.
The technical solution adopted in the present invention is in the method for the compound silvering of dacron surface preparation titanium dioxide nanoparticle, specifically to implement according to following steps:
Step 1: dacron is carried out pre-treatment;
Step 2: the compound silvering of dacron surface preparation titanium dioxide nanoparticle after the pre-treatment that step 1 obtains.
Characteristics of the present invention also are,
The wherein pre-treatment in the step 1, specifically implement according to following steps:
A. alligatoring, adopt quality-volumetric concentration be the sodium hydroxide solution of 160~240g/L as coarsening solution, dacron is placed in the coarsening solution, be under 45~65 ℃ the condition, to handle 45~70min in temperature, weight-loss ratio is controlled between 8~16%;
B. sensitization activation, dacron after the alligatoring that step a is obtained, be placed in the colloidal pd activation solution, under 45~65 ℃ of conditions of temperature, handled 2~6 hours, it consists of colloidal pd activation solution according to quality-volumetric concentration: palladium bichloride 0.12~0.20g/L, stannous chloride 8~14g/L, hydrochloric acid 8~14g/L, sodium chloride 140~180g/L;
C. dispergation, the dacron after the sensitization activation that step b is obtained is placed on to be separated in the glue, in temperature is under 30~60 ℃ the condition, to handle 1~5min, and separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80~120g/L;
D. reduction, the dacron behind the dispergation that step c is obtained is placed in the reducing solution, at ambient temperature, handles 2~8min, and it is the sodium hypophosphite solution of 10~20g/L that reducing solution adopts quality-volumetric concentration.
Wherein in the step 2 at the compound silvering of dacron surface preparation titanium dioxide nanoparticle, specifically implement according to following steps: according to volume ratio is that 1:1~5 take by weighing nano titanium oxide dispersion and reducing solution, mixes to obtain mixed solution b; Dacron after the pre-treatment that step 1 is obtained is put into silver ammino solution, the fabric addition is at 4~10g in every liter of silver ammino solution, for slowly joining mixed solution b in the silver ammino solution that is impregnated with dacron and constantly, stirs 1:4 by volume, in frequency is that 28~50KHz, power are to carry out the reaction of sonic oscillation plating under the condition of 100~300W, question response finishes back taking-up dacron and cleans with running water, naturally dry, promptly finish at the compound silvering of dacron surface preparation titanium dioxide nanoparticle.
Nano titanium oxide dispersion wherein, specifically be prepared from according to following steps: according to volume ratio is that to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid to 1:1, mix, according to adding 10~30g titanium dioxide nanoparticle in every liter of mixed acid solution, prepare mixed solution a, is 50KHz with mixed solution a in frequency, power is sonic oscillation 10~30min under the condition of 100W, use in the sodium hydroxide solution then and residual acid, and to clean repeatedly to solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry obtain the good titanium dioxide nanoparticle of preliminary treatment; According to volume ratio is that 1:1 mixes polyvinylpyrrolidone with Tween 80, make that the quality-volumetric concentration of mixed solution is 2g/L, add the good titanium dioxide nanoparticle of preliminary treatment to mixed solution, make nano titanium oxide concentration, obtain nano titanium oxide dispersion at 1.0~2.0g/L.
Silver ammino solution wherein, specifically be prepared from: take by weighing the liquor argenti nitratis ophthalmicus of 10~40g/L and the potassium hydroxide solution of 10~20g/L according to quality-volumetric concentration according to following steps, slowly dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, then slowly add potassium hydroxide solution to there being the pitchy precipitation to generate, add ammonia spirit again till precipitate the clarification of complete solvent soln, obtain silver ammino solution.
Reducing solution wherein specifically is prepared from according to following steps: glucose is dissolved in deionized water and constantly stirring, makes that the quality-volumetric concentration of glucose is 8~25g/L, obtain reducing solution.
The invention has the beneficial effects as follows; on the basis of traditional chemical silver plating process; at the easy shortcoming of reuniting of titanium dioxide nanoparticle; use the ultrasonic dispersing nanometer titanium dioxide granule of dispersant; then it is added in the chemical plating liquid; it is chemically composited silver-plated under the ultrasonic wave condition dacron to be carried out titanium dioxide nanoparticle, has not only improved the anti-wear performance of terylene chemical silvering fabric, and has given chemical silvering fabric photocatalytic activity.
Description of drawings
Fig. 1 is the stereoscan photograph of dacron general chemistry after silver-plated;
Fig. 2 adopts the inventive method that dacron is carried out the chemically composited stereoscan photograph after silver-plated of titanium dioxide nanoparticle;
Fig. 3 is the silver-plated and X-ray diffraction spectrogram contrast of employing the inventive method behind the compound silvering of dacron surface preparation titanium dioxide nanoparticle of dacron general chemistry.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The present invention specifically implements according to following steps in the method for the compound silvering of dacron surface preparation titanium dioxide nanoparticle:
Step 1: dacron pre-treatment
A. alligatoring, adopt quality-volumetric concentration be the sodium hydroxide solution of 160~240g/L as coarsening solution, dacron is placed in the coarsening solution, be under 45~65 ℃ the condition, to handle 45~70min in temperature, weight-loss ratio is controlled between 8~16%.
B. sensitization activation, dacron after the alligatoring that the last step was obtained, be placed in the colloidal pd activation solution, under 45~65 ℃ of conditions of temperature, to handle 2~6 hours, colloidal pd activation solution is according to preparing with the quality-volumetric concentration of water, it consists of: palladium bichloride 0.12~0.20g/L, stannous chloride 8~14g/L, hydrochloric acid 8~14g/L, sodium chloride 140~180g/L.
C. dispergation, the dacron after the sensitization activation that the last step was obtained is placed on to be separated in the glue, in temperature is under 30~60 ℃ the condition, to handle 1~5min, and separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80~120g/L.
D. reduction, the dacron behind the dispergation that the last step was obtained is placed in the reducing solution, at ambient temperature, handles 2~8min.It is the sodium hypophosphite solution of 10~20g/L that reducing solution adopts quality-volumetric concentration.
Step 2: at the compound silvering of dacron surface preparation titanium dioxide nanoparticle
The preparation of nano titanium oxide dispersion, according to volume ratio is that to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid to 1:1, mix, according to adding 10~30g titanium dioxide nanoparticle in every liter of mixed acid solution, mix and obtain mixed solution a, with mixed solution a sonic oscillation 10~30min under frequency 50KHz, power 100W condition, use in 1 mole the sodium hydroxide solution then and residual acid, and to clean repeatedly to solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry obtain the good titanium dioxide nanoparticle of preliminary treatment.The dose volume ratio is polyvinylpyrrolidone and the Tween 80 mixed solution of 2g/L for the concentration of 1:1, and to wherein adding the certain amount of nano titanium dioxide granule, makes nano titanium oxide concentration at 1.0~2.0g/L.
The preparation silver ammino solution, take by weighing the liquor argenti nitratis ophthalmicus of 10~40g/L, the potassium hydroxide solution of 10~20g/L according to quality-volumetric concentration, slowly dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, then slowly adding potassium hydroxide solution has the pitchy precipitation to generate, add ammonia spirit again till precipitate the clarification of complete solvent soln, prepare silver ammino solution.
The preparation reducing solution is dissolved in deionized water and constantly stirring with glucose, makes that the quality-volumetric concentration of glucose is 8~25g/L.
According to volume ratio is that 1:1~5 take by weighing nano titanium oxide dispersion and reducing solution, mixes to obtain mixed solution b; The dacron that preliminary treatment is good is put into silver ammino solution, the fabric addition is at 4~10g in every liter of silver ammino solution, 1:4 slowly joins mixed solution b in the silver ammino solution that is impregnated with dacron and constantly and stirs by volume, carries out the reaction of sonic oscillation plating under frequency 28~50KHz, power 100~300W condition.Question response finishes back taking-up dacron to be cleaned with running water, dries naturally, promptly finishes at the compound silvering of dacron surface preparation titanium dioxide nanoparticle.
Fig. 1 and Fig. 2 are respectively the silver-plated and chemically composited silver-plated stereoscan photographs of titanium dioxide nanoparticle of dacron general chemistry.As can be seen, the compound silver coating fabric coating surface of the silver-plated ratio nano titanium dioxide granule of general chemistry is level and smooth, the particle that the compound silver coating fabric coating surface of titanium dioxide nanoparticle distributes and differs in size, the nano titanium oxide composite silver coating is ripples shape under the ultrasonic wave condition, many small pores that distributing, surperficial floccule obviously reduces.Fig. 3 is the silver-plated and compound silver-plated X-ray diffraction spectrogram of titanium dioxide nanoparticle of dacron general chemistry.Test result shows, add after the titanium dioxide nanoparticle in the chemical plating liquid, crystallite dimension increases to some extent, and it is fine and close more that coating becomes, wherein the grain size at general chemistry silver-plated (111) crystal face place is 16.4nm, and the compound silver-plated grain size of titanium dioxide nanoparticle is 24.1nm.
According to standard GB/T 21196.3-2007 " mensuration the 3rd part of textiles Martindale fabric abrasion resistance: mass loss determine " and GB/T 21196.4-2007 " mensuration the 4th part of textiles Martindale fabric abrasion resistance: the evaluation of appearance change ", detect the anti-wear performance of common silver-plated and the compound silver coating fabric of titanium dioxide nanoparticle.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7 g.When rate of body weight gain 15~30% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 1.5~3.6%, and the mass loss rate of the compound silver coating fabric of titanium dioxide nanoparticle is 0.8~2.1%; When fabric reaches friction during terminal point, the diffusive that promptly the adds up area that comes off fully reaches 1/3rd when above, and common silver coating fabric friction number of times is 800~1200 times, and the compound silver coating fabric of the nano titanium oxide number of times that rubs is 1200~1600 times.
The methylene orange solution 20mL of preparation 20mg/L, (sample size 4.5cm * 5cm) places methylene orange solution with fabric to be measured, with quartz ultraviolet lamp (power 20W, dominant wavelength 254nm) carries out irradiation apart from liquid level 10cm, measure the absorbance A of solution every 10min with the UV-1600 ultraviolet-uisible spectrophotometer at the 462nm place, according to the concentration C of Lambert-Beer's law calculating solution, computational methods are seen formula (1):
A=K
462nm×C=0.0641×C (1)
Computational methods to methylene orange dyestuff photocatalytic degradation rate D are seen formula (2):
D=(C
1-C
2)/C
1? (2)
In the formula, C
1And C
2Be respectively the forward and backward concentration (mg/L) of methylene orange solution ultraviolet irradiation.Through the ultraviolet irradiation of 90min, the degradation rate of general chemistry silver coating fabric is 70~82%, and the degradation rate of the compound silver coating fabric of titanium dioxide nanoparticle is 78~90%.
Beneficial effect of the present invention place is described from the principle aspect:
1. the present invention adopts titanium dioxide nanoparticle, controls its quality-volumetric concentration at 1.0~2.0g/L.When greater than this scope, titanium dioxide nanoparticle concentration is excessive, and the nano particle showed increased that is contained in the unit volume in the solution very easily causes reunion, forms precipitation; When less than this scope, the nano-dispersed liquid measure of adding is just more relatively, destroys the plating bath internal environment easily, influences the chemical silvering reaction and normally carries out.
2. nano dispersion fluid and reducing solution volume ratio are 1:1~5, and when less than this scope, the nano-dispersed liquid hold-up increases relatively, and the titanium dioxide nanoparticle consumption increases, and wasting phenomenon is more serious, and bath stability reduces simultaneously, influences normal plating; When greater than this scope, the nano titanium oxide consumption reduces relatively, be deposited in the coating nano-particle content seldom, do not reach the purpose that changes coating structure.
3. to adopt silver ammino solution and reducing solution to carry out titanium dioxide nanoparticle under the ultrasonic wave condition chemically composited silver-plated in the present invention, when in frequency 28~50KHz, power 100~300W condition following time, and gained silvering well-formed, overlay coating is even; When less than this scope, do not have the silver-plated effect of sonic oscillation assistant chemical; When greater than this scope, plating speed can be affected, and the plating leakage phenomenon appears in the fabric face part.
Embodiment 1
The dacron pre-treatment: with the NaOH of 160g/L, handle dacron 45min under 45 ℃ of conditions, the control mass loss rate is about 8%; Use the 0.12g/L palladium bichloride, the 8g/L stannous chloride, 8g/L hydrochloric acid, the solution of 140g/L sodium chloride was handled dacron 2 hours under 45 ℃ of conditions; Under 30 ℃ of conditions, handle dacron 1min with 80g/L hydrochloric acid; Handle dacron 2min at ambient temperature with the 10g/L sodium hypophosphite.The preparation of nano titanium oxide dispersion: the 10g titanium dioxide nanoparticle is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1, sonic oscillation 10min under 50KHz, 100W condition, neutralize with sodium hydroxide solution then, and to clean repeatedly until solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry; Cleaned titanium dioxide nanoparticle is dispersed in the polyvinylpyrrolidone and Tween 80 mixed solution of 2g/L volume ratio 1:1, is mixed with the nano titanium oxide dispersion of 1g/L.The preparation of silver ammino solution: take by weighing the silver nitrate of 10g, the potassium hydroxide of 10g, be dissolved in respectively in the deionized water of 300mL; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, and then slowly adding potassium hydroxide solution has the pitchy precipitation to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; And additional deionized water promptly obtains silver ammino solution to 1L.The preparation of reducing solution: take by weighing the glucose of 8g, be dissolved in the deionized water of 1L.The dacron titanium dioxide nanoparticle is chemically composited silver-plated: according to volume ratio is 1:1, nano titanium oxide dispersion is mixed with reducing solution and ceaselessly stirring; By fabric addition 4g in every liter of silver ammino solution, the dacron that preliminary treatment is good is put into silver ammino solution; 1:4 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly stirring by volume again, and sonic oscillation carries out the plating reaction under 28KHz, 100W condition.Question response finishes the back and takes out dacron running water washes clean, dries naturally.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of the common silver-plated and compound silver coating fabric of titanium dioxide nanoparticle.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 15% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 1.5%, and the mass loss rate of the compound silver coating fabric of titanium dioxide nanoparticle is 0.8%; When fabric reached the friction terminal point, common silver coating fabric friction number of times was 870 times, and the compound silver coating fabric friction of titanium dioxide nanoparticle number of times is 1250 times.Photocatalytic degradation methylene orange dyestuff result shows that through the ultraviolet irradiation of 90min, the degradation rate of general chemistry silver coating fabric is 71.6%, and the degradation rate of the compound silver coating fabric of titanium dioxide nanoparticle is 78.2%.
Embodiment 2
The dacron pre-treatment: with the NaOH of 240g/L, handle dacron 70min under 65 ℃ of conditions, the control mass loss rate is about 16%; Use the 0.2g/L palladium bichloride, the 14g/L stannous chloride, 14g/L hydrochloric acid, 180g/L sodium chloride was handled dacron 6 hours under 65 ℃ of conditions; Use 120g/L hydrochloric acid, under 60 ℃ of conditions, handle dacron 5min; Handle dacron 8min at ambient temperature with the 20g/L sodium hypophosphite.The preparation of nano titanium oxide dispersion: the 30g titanium dioxide nanoparticle is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1, sonic oscillation 30min under 50KHz, 100W condition, neutralize with 1 molar sodium hydroxide solution then, and to clean repeatedly until solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry; Cleaned titanium dioxide nanoparticle is dispersed in the polyvinylpyrrolidone and Tween 80 mixed solution of 2g/L volume ratio 1:1, is mixed with the nano titanium oxide dispersion of 2g/L.The preparation of silver ammino solution: take by weighing the silver nitrate of 40g, the potassium hydroxide of 20g, be dissolved in respectively in the deionized water of 400mL; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, and then slowly adding potassium hydroxide solution has the pitchy precipitation to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; And additional deionized water promptly obtains silver ammino solution to 1L.The preparation of reducing solution: take by weighing 25g glucose, be dissolved in the deionized water of 1L.The dacron titanium dioxide nanoparticle is chemically composited silver-plated: according to volume ratio is that 1:5 mixes nano titanium oxide dispersion and ceaselessly stirring with reducing solution; By fabric addition 10g in every liter of silver ammino solution, the dacron that preliminary treatment is good is put into silver ammino solution; 1:4 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly and stirs sonic oscillation plating reaction under 50KHz, 300W condition by volume again.Question response finishes the back and takes out dacron running water washes clean, dries naturally.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of the common silver-plated and compound silver coating fabric of titanium dioxide nanoparticle.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 30% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 3.6%, and the mass loss rate of the compound silver coating fabric of titanium dioxide nanoparticle is 2.1%; When fabric reached the friction terminal point, common silver coating fabric friction number of times was 1190 times, and the compound silver coating fabric friction of titanium dioxide nanoparticle number of times is 1580 times.Photocatalytic degradation methylene orange dyestuff result shows that through the ultraviolet irradiation of 90min, the degradation rate of general chemistry silver coating fabric is 80.2%, and the degradation rate of the compound silver coating fabric of titanium dioxide nanoparticle is 89.8%.
Embodiment 3
The dacron pre-treatment: with the NaOH of 200g/L, handle dacron 60min under 50 ℃ of conditions, the control mass loss rate is about 12%; Use the 0.16g/L palladium bichloride, the 12g/L stannous chloride, 12g/L hydrochloric acid, 160g/L sodium chloride was handled dacron 5 hours under 60 ℃ of conditions; Under 45 ℃ of conditions, handle dacron 2min with 100g/L hydrochloric acid; Handle dacron 5min at ambient temperature with the 15g/L sodium hypophosphite.The preparation of nano titanium oxide dispersion: the 15g titanium dioxide nanoparticle is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1, sonic oscillation 20min under 50KHz, 100W condition, neutralize with 1 molar sodium hydroxide solution then, and to clean repeatedly to solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry; Cleaned titanium dioxide nanoparticle is dispersed in the polyvinylpyrrolidone and Tween 80 mixed solution of 2g/L volume ratio 1:1, is mixed with the nano titanium oxide dispersion of 1.5g/L.The preparation of silver ammino solution:, be dissolved in respectively in the deionized water of 300mL with 30g silver nitrate, 15g NaOH; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, and then slowly adding sodium hydroxide solution has the pitchy precipitation to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; And additional deionized water promptly obtains silver ammino solution to 1L.The preparation of reducing solution: take by weighing the glucose of 15g, be dissolved in the deionized water of 1L.The dacron titanium dioxide nanoparticle is chemically composited silver-plated: according to volume ratio is 1:3, nano titanium oxide dispersion is mixed with reducing solution and ceaselessly stirring; By fabric addition 8g in every liter of silver ammino solution, the dacron that preliminary treatment is good is put into silver ammino solution; 1:4 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly and stirs sonic oscillation plating reaction under 28KHz, 300W condition by volume again.Question response finishes the back and takes out dacron running water washes clean, dries naturally.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of the common silver-plated and compound silver coating fabric of titanium dioxide nanoparticle.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 20% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 2.7%, and the mass loss rate of the compound silver coating fabric of titanium dioxide nanoparticle is 1.6%; When fabric reaches friction during terminal point, the diffusive that promptly the adds up area that comes off fully reaches 1/3rd when above, and common silver coating fabric friction number of times is 1080 times, and the compound silver coating fabric of the nano titanium oxide number of times that rubs is 1450 times.Photocatalytic degradation methylene orange dyestuff result shows that through the ultraviolet irradiation of 90min, the degradation rate of general chemistry silver coating fabric is 75.4%, and the degradation rate of the compound silver coating fabric of titanium dioxide nanoparticle is 86.3%.
The inventive method, use mixed dispersant polyvinylpyrrolidone and Tween 80 supersonic oscillations dispersing nanometer titanium dioxide granule, then it is added in the chemical plating liquid, make titanium dioxide nanoparticle stable dispersion in silver plating liquid, the dacron silvering structure of plating is fine and close more, has improved the photocatalytically degradating organic dye ability of terylene chemical silvering fabric.
Claims (6)
1. in the method for the compound silvering of dacron surface preparation titanium dioxide nanoparticle, it is characterized in that, specifically implement according to following steps:
Step 1: dacron is carried out pre-treatment;
Step 2: the compound silvering of dacron surface preparation titanium dioxide nanoparticle after the pre-treatment that step 1 obtains.
2. the method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle according to claim 1 is characterized in that, the pre-treatment in the described step 1 is specifically implemented according to following steps:
A. alligatoring, adopt quality-volumetric concentration be the sodium hydroxide solution of 160~240g/L as coarsening solution, dacron is placed in the coarsening solution, be under 45~65 ℃ the condition, to handle 45~70min in temperature, weight-loss ratio is controlled between 8~16%;
B. sensitization activation, dacron after the alligatoring that step a is obtained, be placed in the colloidal pd activation solution, under 45~65 ℃ of conditions of temperature, handled 2~6 hours, it consists of colloidal pd activation solution according to quality-volumetric concentration: palladium bichloride 0.12~0.20g/L, stannous chloride 8~14g/L, hydrochloric acid 8~14g/L, sodium chloride 140~180g/L;
C. dispergation, the dacron after the sensitization activation that step b is obtained is placed on to be separated in the glue, in temperature is under 30~60 ℃ the condition, to handle 1~5min, and separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80~120g/L;
D. reduction, the dacron behind the dispergation that step c is obtained is placed in the reducing solution, at ambient temperature, handles 2~8min, and it is the sodium hypophosphite solution of 10~20g/L that reducing solution adopts quality-volumetric concentration.
3. the method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle according to claim 1, it is characterized in that, in the described step 2 at the compound silvering of dacron surface preparation titanium dioxide nanoparticle, specifically implement according to following steps: according to volume ratio is that 1:1~5 take by weighing nano titanium oxide dispersion and reducing solution, mixes to obtain mixed solution b; Dacron after the pre-treatment that step 1 is obtained is put into silver ammino solution, the fabric addition is at 4~10g in every liter of silver ammino solution, for slowly joining mixed solution b in the silver ammino solution that is impregnated with dacron and constantly, stirs 1:4 by volume, in frequency is that 28~50KHz, power are to carry out the reaction of sonic oscillation plating under the condition of 100~300W, question response finishes back taking-up dacron and cleans with running water, naturally dry, promptly finish at the compound silvering of dacron surface preparation titanium dioxide nanoparticle.
4. the method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle according to claim 3, it is characterized in that, described nano titanium oxide dispersion, specifically be prepared from according to following steps: according to volume ratio is that to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid to 1:1, mix, according to adding 10~30g titanium dioxide nanoparticle in every liter of mixed acid solution, prepare mixed solution a, is 50KHz with mixed solution a in frequency, power is sonic oscillation 10~30min under the condition of 100W, use in the sodium hydroxide solution then and residual acid, and to clean repeatedly to solution with deionized water be neutral, vacuum filtration, 80 ℃ of oven dry obtain the good titanium dioxide nanoparticle of preliminary treatment; According to volume ratio is that 1:1 mixes polyvinylpyrrolidone with Tween 80, make that the quality-volumetric concentration of mixed solution is 2g/L, add the good titanium dioxide nanoparticle of preliminary treatment to mixed solution, make nano titanium oxide concentration, obtain nano titanium oxide dispersion at 1.0~2.0g/L.
5. the method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle according to claim 3, it is characterized in that, described silver ammino solution, specifically be prepared from: take by weighing the liquor argenti nitratis ophthalmicus of 10~40g/L and the potassium hydroxide solution of 10~20g/L according to quality-volumetric concentration according to following steps, slowly dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy precipitation to be generated just is dissolved to solution becomes, then slowly add potassium hydroxide solution to there being the pitchy precipitation to generate, add ammonia spirit again till precipitate the clarification of complete solvent soln, obtain silver ammino solution.
6. the method at the compound silvering of dacron surface preparation titanium dioxide nanoparticle according to claim 3, it is characterized in that, described reducing solution, specifically be prepared from: glucose is dissolved in deionized water and constantly stirring according to following steps, make that the quality-volumetric concentration of glucose is 8~25g/L, obtain reducing solution.
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